CN103803570A - Method for changing color of attapulgite by using solvothermal reaction - Google Patents
Method for changing color of attapulgite by using solvothermal reaction Download PDFInfo
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- CN103803570A CN103803570A CN201410071113.0A CN201410071113A CN103803570A CN 103803570 A CN103803570 A CN 103803570A CN 201410071113 A CN201410071113 A CN 201410071113A CN 103803570 A CN103803570 A CN 103803570A
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Abstract
The invention provides a method for changing the color of attapulgite by using solvothermal reaction. The method comprises the following steps: stirring and dispersing erythrine attapulgite clay subjected to acid treatment in a dimethylsulfoxide solvent according to a solid-liquid mass ratio being 1:25-1:200, reacting for 4-48 hours at the temperature of 120-200 DEG C, carrying out centrifugal separation, and drying, thus obtaining the creamy white attapulgite. According to the method, S=O group in dimethylsulfoxide interacts with the attapulgite and acts on ferric iron in an attapulgite skeleton so as to realize the change of color of the attapulgite. Meanwhile, the transition of iron valence state changes the structure charge of the attapulgite, so that the adsorption capacity of the attapulgite clay is improved, and a new approach is opened up for application of the erythrine attapulgite clay abundant in our country. In addition, the method is simple in process, easy to control and low in cost, has low requirements on equipment and facilitates industrial production.
Description
Technical field
The present invention relates to a kind of method of utilizing solvent thermal reaction to change attapulgite color, relate in particular to a kind of dimethylsulfoxide solvent thermal response of utilizing and make brick-red attapulgite change the method for rice white attapulgite into, belong to the deep processing of nano silicate material and preparing technical field.
Background technology
Attapulgite clay is a kind of layer silicate mineral containing Shuifu County's magnalium, owing to thering is unique excellent crystalline form looks, micropore canals, the larger advantage such as specific surface area and good absorption property, obtain application at numerous areas such as fine chemistry industry, matrix material, function carrier, petrochemical complex and environmental protection in recent years.China has found the concavo-convex handful stone of large-scale high-quality clay deposit as far back as Anhui two provinces of Soviet Union, afterwards successively in Gansu, the ground such as Sichuan, Guizhou, Henan, Shanxi, Inner Mongol, Hubei, Hebei and Yunnan found a collection of mineral deposit (point) successively, Mineral resources prospect is considerable.Wherein, the concavo-convex handful stone clay ore reserves that Gansu is verified in recent years has 400,000,000 tons more than.But attapulgite is in the process of one-tenth ore deposit, due to Mg
2+shortage cause Mg in octahedral layer
2+there is major part vacancy the position occupying or is Al
3+, Fe
3+or Fe
2+occupied, and a large amount of Fe
3+occupy that attapulgite is presented is brick-red.In the concavo-convex handful stone clay of Anhui two provinces of Soviet Union, the content of concavo-convex handful stone is relatively high, and color is white or rice white simultaneously, because researching and developing comparatively system, has formed at present industrial colony.And the concavo-convex handful stone clay ore deposit in other area does not have sizable application, except the content of concavo-convex handful stone is relatively not high, be mainly that the color and luster in concavo-convex handful stone clay ore deposit is darker, adsorptive power a little less than, be unfavorable for the exploitation of product.
In order to improve the color and luster of concavo-convex handful stone clay, first CN101423673 carries out dispersion treatment by natural concavo-convex handful stone clay in water, prepares nano concavo-convex and holds in both hands stone dispersion liquid, then with TiCl
4for raw material is prepared Aggregation of Nanometer Titanium Dioxide body, again Aggregation of Nanometer Titanium Dioxide body and nano concavo-convex handful stone are carried out compound, utilize the dissolving with hydrochloric acid that in reaction process, titanium tetrachloride hydrolysis produces to go out the ferro element in concavo-convex handful stone, finally carry out complexing deironing with sodium oxalate.CN102660158A also utilizes aluminium hydroxide and pure aluminium silicate synergic whitening modification dolomite/concavo-convex handful stone.These methods no doubt can play the effect that concavo-convex handful stone brightens, but itself do not brighten from concavo-convex handful stone structure.Thereby explore new method of whitening, the utilization of the abundant brick-red concavo-convex handful stone clay of China's reserves is had important practical significance.
Summary of the invention
The object of this invention is to provide a kind of method of utilizing solvent thermal reaction to change attapulgite clay color, for new approach is opened up in the utilization of brick-red concavo-convex handful stone clay.
The present invention utilizes solvent thermal reaction to change the method for attapulgite color, be by the brick-red attapulgite clay after acid treatment by the mass/volume of 1:25～1:200 than dispersed with stirring in dimethylsulfoxide solvent, under the condition of 120～200 ℃, react 4～48h, centrifugation, dry, obtain rice white attapulgite.
The present invention utilizes the S=O group in methyl-sulphoxide, realizes the interaction of S=O group and attapulgite under hyperbaric environment condition, by with attapulgite skeleton in ferric effect, realize the transformation of attapulgite color and luster.Simultaneously the changing of transformation of iron valence state the structure charge of attapulgite, thereby improved attapulgite clay adsorptive power.Measuring, the rice white attapulgite clay that the present invention changes after color has improved more than 2 times the loading capacity of methylene blue.
The acid treatment process of brick-red attapulgite clay is: by pulverize brick-red attapulgite clay by the mass/volume of 1:10～1:50 than being dispersed in the acid solution (sulfuric acid or hydrochloric acid) of mass concentration 1～10%, stir 1～4h, mistake 200 mesh sieves remove impurity; After centrifugation, be washed with water to pH=5～6, dry, pulverize and get final product.Acid-treated effect is: one side is decomposed the impurity such as the carbonate of attapulgite clay association; The duct that can further dredge on the other hand attapulgite clay, is conducive to the interaction of attapulgite and methyl-sulphoxide.
Dimethylsulfoxide solvent used can be recycled, and can reduce production costs.
In sum, the present invention is by dimethylsulfoxide solvent thermal response, realizing brick-red attapulgite in the transformation of white attapulgite, effectively improve the adsorptive power of attapulgite, for new way has been opened up in the application of the abundant brick-red attapulgite clay of China's reserves.In addition, technique of the present invention is simple, is easy to control, and not high to equipment requirements, cost is low, is conducive to suitability for industrialized production.
Embodiment
The method that solvent thermal reaction of the present invention is changed to attapulgite clay color below by specific embodiment is described further.
embodiment 1
Under agitation condition, it is in 5% sulphuric acid soln that brick-red 20g attapulgite clay is dispersed in to 200mL mass concentration, stirs to cross 200 mesh sieves after 2h and remove the impurity such as quartz sand; After centrifugation, be washed with water to pH=6, then at 105 ℃, dry 4h, pulverize, cross 200 mesh sieves, obtain acid treatment attapulgite clay.
Acid treatment attapulgite clay is dispersed in 600 mL methyl-sulphoxides, stirs 30min, be uniformly dispersed and be placed in 1 L autoclave, be at 180 ℃, to react 12 h in temperature, naturally centrifugation after cooling is then dried 4h at 105 ℃, obtains rice white attapulgite.
embodiment 2
Under agitation condition, it is in 10% sulphuric acid soln that brick-red 15g attapulgite clay is dispersed in to 200mL mass concentration, stirs to cross 200 mesh sieves after 2h and remove the impurity such as quartz sand; After centrifugation, be washed with water to pH=5, then at 105 ℃, dry 4h, pulverize, cross 200 mesh sieves, obtain acid treatment attapulgite clay.
Acid treatment attapulgite clay is dispersed in 600 mL methyl-sulphoxides, stirs 30 min, be uniformly dispersed and be placed in 1 L autoclave, be at 160 ℃, to react 24 h in temperature, after naturally lowering the temperature, centrifugation, at 105 ℃, dry after 4h, obtain rice white attapulgite.
embodiment 3
Under agitation condition, it is in 10% hydrochloric acid soln that brick-red 15g attapulgite clay is dispersed in to 200mL mass concentration, after stirring 2h, cross 200 mesh sieves and remove the impurity such as quartz sand, after centrifugation, be washed with water to pH value=6, then after drying 4h at 105 ℃, pulverize 200 mesh sieves, obtained acid treatment attapulgite clay.
Acid treatment attapulgite clay is dispersed in 600 mL methyl-sulphoxides, stirs 30 min, be uniformly dispersed and be placed in 1 L autoclave, be at 200 ℃, to react 6 h in temperature, after naturally lowering the temperature, centrifugation, at 105 ℃, dry after 4h, obtain rice white attapulgite.
embodiment 4
Under agitation condition, it is in 8% sulphuric acid soln that brick-red 10g attapulgite clay is dispersed in to 200mL mass concentration, after stirring 2h, cross 200 mesh sieves and remove the impurity such as quartz sand, after centrifugation, be washed with water to pH value=6, then after drying 4h at 105 ℃, pulverize 200 mesh sieves, obtained acid treatment attapulgite clay.
Acid treatment attapulgite clay is dispersed in 600 mL methyl-sulphoxides, stirs 30 min, be uniformly dispersed and be placed in 1 L autoclave, be at 150 ℃, to react 6 h in temperature, after naturally lowering the temperature, centrifugation, at 105 ℃, dry after 4h, obtain rice white attapulgite.
Claims (4)
1. utilize solvent thermal reaction to change the method for attapulgite color, be by the brick-red attapulgite clay dispersed with stirring after acid treatment in dimethylsulfoxide solvent, under the condition of 120～200 ℃, react 4～48h, centrifugation, dry, obtain rice white attapulgite.
2. utilize as claimed in claim 1 solvent thermal reaction to change the method for attapulgite color, it is characterized in that: the acid treatment process of brick-red attapulgite clay is: by pulverize brick-red attapulgite clay by the mass/volume of 1:10～1:50 than being scattered in the acid solution of mass concentration 1～10%, stir 1～4h, cross 200 mesh sieves and remove impurity; After centrifugation, be washed with water to pH=5～6, dry, pulverize and get final product.
3. utilize as claimed in claim 1 or 2 solvent thermal reaction to change the method for attapulgite color, it is characterized in that: brick-red attapulgite clay is 1:25～1:200 with the mass/volume ratio of dimethylsulfoxide solvent.
4. utilize as claimed in claim 1 or 2 solvent thermal reaction to change the method for attapulgite color, it is characterized in that: described acid solution is sulphuric acid soln or hydrochloric acid soln.
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| CN103803570B CN103803570B (en) | 2016-06-22 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105802282A (en) * | 2016-02-29 | 2016-07-27 | 中国科学院兰州化学物理研究所 | Method for preparing red hybridized pigment from red attapulgite clay |
| CN110078086A (en) * | 2019-06-04 | 2019-08-02 | 南京信息工程大学 | A kind of purification of low-grade red attapulgite stone clay and decoloring process |
| CN115073938A (en) * | 2022-06-23 | 2022-09-20 | 河西学院 | Preparation method, product and application of attapulgite/cobalt blue hybrid pigment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423673A (en) * | 2008-11-28 | 2009-05-06 | 江苏工业学院 | Method for improving brightness of attapulgite |
| CN101818000A (en) * | 2009-03-14 | 2010-09-01 | 兰州理工大学 | Method for removing iron and whitening for iron-containing attapulgite clay |
| CN102649573A (en) * | 2011-02-24 | 2012-08-29 | 中国科学院兰州化学物理研究所 | Preparation method for improving aggregation of attapulgite clay nanometer material |
| CN102660158A (en) * | 2012-04-12 | 2012-09-12 | 盱眙华洪矿业有限公司 | Dolomite/attapulgite composition and preparation method thereof |
-
2014
- 2014-02-28 CN CN201410071113.0A patent/CN103803570B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423673A (en) * | 2008-11-28 | 2009-05-06 | 江苏工业学院 | Method for improving brightness of attapulgite |
| CN101818000A (en) * | 2009-03-14 | 2010-09-01 | 兰州理工大学 | Method for removing iron and whitening for iron-containing attapulgite clay |
| CN102649573A (en) * | 2011-02-24 | 2012-08-29 | 中国科学院兰州化学物理研究所 | Preparation method for improving aggregation of attapulgite clay nanometer material |
| CN102660158A (en) * | 2012-04-12 | 2012-09-12 | 盱眙华洪矿业有限公司 | Dolomite/attapulgite composition and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105802282A (en) * | 2016-02-29 | 2016-07-27 | 中国科学院兰州化学物理研究所 | Method for preparing red hybridized pigment from red attapulgite clay |
| CN105802282B (en) * | 2016-02-29 | 2018-01-30 | 中国科学院兰州化学物理研究所 | The method for preparing red hybrid pigment using red attapulgite stone clay |
| CN110078086A (en) * | 2019-06-04 | 2019-08-02 | 南京信息工程大学 | A kind of purification of low-grade red attapulgite stone clay and decoloring process |
| CN115073938A (en) * | 2022-06-23 | 2022-09-20 | 河西学院 | Preparation method, product and application of attapulgite/cobalt blue hybrid pigment |
| CN115073938B (en) * | 2022-06-23 | 2024-04-23 | 河西学院 | Preparation method, product and application of attapulgite/cobalt blue hybrid pigment |
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| CN103803570B (en) | 2016-06-22 |
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